CN108417789A - A kind of MoS for negative electrode of lithium ion battery2/ C microballoon composite material and preparation methods - Google Patents
A kind of MoS for negative electrode of lithium ion battery2/ C microballoon composite material and preparation methods Download PDFInfo
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- CN108417789A CN108417789A CN201810088512.6A CN201810088512A CN108417789A CN 108417789 A CN108417789 A CN 108417789A CN 201810088512 A CN201810088512 A CN 201810088512A CN 108417789 A CN108417789 A CN 108417789A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of MoS for negative electrode of lithium ion battery2/ C microballoon composite material and preparation methods are related to technical field of lithium ion, and the composite material is combined by molybdenum disulfide and carbosphere, and the molybdenum disulfide is grown in carbosphere surface；Preparation method includes the following steps：The aqueous solution of saccharide compound is prepared, is then added in hydrothermal reaction kettle and carries out hydro-thermal reaction, be cooled to room temperature, centrifugation drying obtains carbosphere；Into carbosphere plus water, sodium molybdate, thiocarbamide is added in stirring thereto, and stirring is transferred in hydrothermal reaction kettle and carries out hydro-thermal reaction, is cooled to room temperature, centrifugal drying, then carry out in an inert atmosphere quenching treatment to get.The present invention grows molybdenum disulfide on its basis again by first preparing carbosphere, on the one hand the electric conductivity of molybdenum disulfide is promoted by introducing carbosphere, on the other hand by the way that molybdenum disulfide is limited its volume expansion caused when being used as lithium ion battery negative material charge and discharge in growth in carbon ball.
Description
Technical field
The present invention relates to technical field of lithium ion battery negative more particularly to a kind of for negative electrode of lithium ion battery
MoS2/ C microballoon composite material and preparation methods.
Background technology
Lithium ion battery is because of superiority such as energy density is big, memory-less effect, specific capacity height, operating voltage height, long lifespans
Matter is widely used in the fields such as energy storage device such as electronic equipment, power battery at present.Current commercialized lithium-ion electric
It is graphite that pond negative material, which uses at most, but the theoretical specific capacity of graphite only has 372mAh/g, and lower specific capacity limits
Lithium ion battery is further applied power battery field.
Molybdenum disulfide is a kind of two-dimensional layer material with similar sandwich structure, in the structure composition of molybdenum disulfide
In, upper layer and lower layer is all made of sulphur atom interconnection respectively, is made of molybdenum atom between this two layers of sulphur atom layer
One layer of atomic layer.Interlamellar spacing wherein between sulphur atom layer and molybdenum courtyard layer is about 0.65nm, much larger than the half of lithium ion
Diameter 0.076nm, this carries out embedded and abjection in molybdenum disulfide interlayer for lithium ion and provides possibility, layer of molybdenum-disulfide and layer it
Between its be connected by Van der Waals force, due to transition metal element have undersaturated d tracks, band gap 1.8eV, this
It is set to show the property of excellent electricity and magnetics.According to this special architectural characteristic of molybdenum disulfide, molybdenum disulfide at present
It is widely used in the fields such as lithium ion battery electrode material, lubricant, catalyst, aerospace.However, using only two sulphur
When changing negative material of this material of molybdenum as lithium ion battery, due to its electric conductivity is bad and in charge and discharge process
Lithium ion insertion repeatedly and abjection cause volume expansion, eventually lead to the decline of its cycle performance.
Invention content
Technical problems based on background technology, the present invention propose a kind of MoS for negative electrode of lithium ion battery2/C
The composite material is used for lithium ion battery negative material, two sulphur can be effectively relieved by microballoon composite material and preparation method
Change molybdenum caused volume expansion in charge and discharge process.
A kind of MoS for negative electrode of lithium ion battery proposed by the present invention2/ C microballoon composite materials, the composite material are
It is combined by molybdenum disulfide and carbosphere, the molybdenum disulfide is grown in carbosphere surface.
The invention also provides the above-mentioned MoS for negative electrode of lithium ion battery2The preparation method of/C microballoon composite materials, packet
Include following steps：
S1, the aqueous solution for preparing saccharide compound；
S2, the aqueous solution of saccharide compound is added in hydrothermal reaction kettle, is placed in Muffle furnace and carries out hydro-thermal reaction, reacted
After be cooled to room temperature, centrifugation drying, obtain carbosphere；
S3, add water, stirring that sodium molybdate, thiocarbamide are added thereto into carbosphere, stirring is transferred in hydrothermal reaction kettle
Hydro-thermal reaction is carried out, is cooled to room temperature after reaction, centrifugal drying obtains MoS2/ C microballoon composite material crude products；
S4, in an inert atmosphere, by MoS2/ C microballoon composite materials carry out quenching treatment to get the flower-shaped MoS of micron order2/
C microballoon composite materials.
Preferably, in the S1, saccharide compound is any one in glucose, fructose, sucrose.
Preferably, in the S1, the mass concentration of saccharide compound aqueous solution is 0.5-2%.
Preferably, in the S2, hydrothermal temperature is 120-180 DEG C, reaction time 5-10h.
Preferably, in the S3, into carbosphere plus water is configured to the solution that mass concentration is 0.5-5%.
Preferably, in the S3, the mass ratio of sodium molybdate and thiocarbamide is 50-150：100-500.
Preferably, in the S3, thermal response temperature is 150-240 DEG C, reaction time 10-15h.
Preferably, in the S4, hardening heat is 300-1000 DEG C, cool time 0.5-5h.
Preferably, in the S4, quenching is tube furnace with device.
Advantageous effect：The invention discloses a kind of MoS for negative electrode of lithium ion battery2/ C microballoon composite materials are first
Carbosphere is prepared, then grows molybdenum disulfide on carbosphere, the electric conductivity of molybdenum disulfide is on the one hand promoted by introducing carbosphere,
On the other hand drawn by the way that molybdenum disulfide is limited it when being used as lithium ion battery negative material charge and discharge in growth in carbon ball
The volume expansion risen.By MoS2When/C microballoon composite materials are used for cell negative electrode material, compared to pure two sulphur not compound with carbon
Change molybdenum, for specific capacity up to 1500mAh/g, capacity boost is apparent, through the molybdenum disulfide compound with carbosphere after cycle 100 weeks
Capacity retention ratio is 90% or more, and compound not with carbosphere its capacity retention ratio of pure molybdenum disulfide is only 50% or so.
Description of the drawings
Fig. 1 is MoS prepared by the embodiment of the present invention 12The SEM of/C microballoon composite materials schemes；
Fig. 2 is MoS prepared by the embodiment of the present invention 22The SEM of/C microballoon composite materials schemes.
Specific implementation mode
In the following, technical scheme of the present invention is described in detail by specific embodiment.
Embodiment 1
The glucose for weighing 500mg is positioned among beaker, and the distilled water that graduated cylinder measures 60mL is used in combination to be positioned over above-mentioned burning
In cup, it is transferred in the hydrothermal reaction kettle of 100mL and is tightened after stirring evenly；Above-mentioned hydrothermal reaction kettle is positioned over Muffle
In stove, 5h is kept the temperature at a temperature of 120 DEG C, is cooled to room temperature after reaction, carbosphere is obtained through centrifugation drying；By carbosphere
It is added in beaker, and distilled water appropriate is added, be configured to a concentration of 0.5% solution, weigh 50mg sodium molybdates, 100mg sulphur
Urea is positioned in above-mentioned sample, is positioned in hydrothermal reaction kettle after stirring evenly, and 10h, reaction knot are kept the temperature at a temperature of 150 DEG C
Beam postcooling obtains MoS to room temperature after centrifugal drying2/ C microballoon composite material crude products, are placed in tube furnace,
5h is kept the temperature at a temperature of 300 DEG C, quenching treatment is carbonized to get the flower-shaped MoS of micron order2/ C microballoon composite materials.
Embodiment 2
The glucose for weighing 800mg is positioned among beaker, and the distilled water that graduated cylinder measures 90mL is used in combination to be positioned over above-mentioned burning
In cup, it is transferred in the hydrothermal reaction kettle of 100mL and is tightened after stirring evenly；Above-mentioned hydrothermal reaction kettle is positioned over Muffle
In stove, 10h is kept the temperature at a temperature of 180 DEG C, is cooled to room temperature after reaction, carbosphere is obtained through centrifugation drying；Carbon is micro-
Ball is added in beaker, and distilled water appropriate is added, and is configured to a concentration of 5% solution, weighs 150mg sodium molybdates, 500mg sulphur
Urea is positioned in above-mentioned sample, is positioned in hydrothermal reaction kettle after stirring evenly, and 15h, reaction knot are kept the temperature at a temperature of 240 DEG C
Beam postcooling obtains MoS to room temperature after centrifugal drying2/ C microballoon composite material crude products, are placed in tube furnace,
4h is kept the temperature at a temperature of 650 DEG C, quenching treatment is carbonized to get the flower-shaped MoS of micron order2/ C microballoon composite materials.
Embodiment 3
The glucose for weighing 1000mg is positioned among beaker, and the distilled water that graduated cylinder measures 80mL is used in combination to be positioned over above-mentioned burning
In cup, it is transferred in the hydrothermal reaction kettle of 100mL and is tightened after stirring evenly；Above-mentioned hydrothermal reaction kettle is positioned over Muffle
In stove, 8h is kept the temperature at a temperature of 160 DEG C, is cooled to room temperature after reaction, carbosphere is obtained through centrifugation drying；By carbosphere
It is added in beaker, and distilled water appropriate is added, be configured to a concentration of 3% solution, weigh 100mg sodium molybdates, 300mg thiocarbamides
It is positioned in above-mentioned sample, is positioned in hydrothermal reaction kettle after stirring evenly, keep the temperature 12h at a temperature of 180 DEG C, reaction terminates
Postcooling obtains MoS to room temperature after centrifugal drying2/ C microballoon composite material crude products, are placed in tube furnace, 700
2h is kept the temperature at a temperature of DEG C, quenching treatment is carbonized to get the flower-shaped MoS of micron order2/ C microballoon composite materials.
Embodiment 4
The glucose for weighing 700mg is positioned among beaker, and the distilled water that graduated cylinder measures 85mL is used in combination to be positioned over above-mentioned burning
In cup, it is transferred in the hydrothermal reaction kettle of 100mL and is tightened after stirring evenly；Above-mentioned hydrothermal reaction kettle is positioned over Muffle
In stove, 8h is kept the temperature at a temperature of 150 DEG C, is cooled to room temperature after reaction, carbosphere is obtained through centrifugation drying；By carbosphere
It is added in beaker, and distilled water appropriate is added, be configured to a concentration of 4% solution, weigh 100mg sodium molybdates, 150mg thiocarbamides
It is positioned in above-mentioned sample, is positioned in hydrothermal reaction kettle after stirring evenly, keep the temperature 12h at a temperature of 220 DEG C, reaction terminates
Postcooling obtains MoS to room temperature after centrifugal drying2/ C microballoon composite material crude products, are placed in tube furnace, 800
1h is kept the temperature at a temperature of DEG C, quenching treatment is carbonized to get the flower-shaped MoS of micron order2/ C microballoon composite materials.
Embodiment 5
The fructose for weighing 1400mg is positioned among beaker, and the distilled water that graduated cylinder measures 70mL is used in combination to be positioned over above-mentioned beaker
In, it is transferred in the hydrothermal reaction kettle of 100mL and is tightened after stirring evenly；Above-mentioned hydrothermal reaction kettle is positioned over Muffle furnace
In, 7h is kept the temperature at a temperature of 160 DEG C, is cooled to room temperature after reaction, carbosphere is obtained through centrifugation drying；By carbosphere plus
Enter in beaker, and distilled water appropriate is added, be configured to a concentration of 2% solution, weigh 80mg sodium molybdates, 200mg thiocarbamides are put
It is placed in above-mentioned sample, is positioned in hydrothermal reaction kettle after stirring evenly, keep the temperature 13h at a temperature of 170 DEG C, after reaction
It is cooled to room temperature, MoS is obtained after centrifugal drying2/ C microballoon composite material crude products, are placed in tube furnace, at 1000 DEG C
At a temperature of keep the temperature 0.5h, quenching treatment is carbonized to get the flower-shaped MoS of micron order2/ C microballoon composite materials.
Embodiment 6
The sucrose for weighing 700mg is positioned among beaker, and the distilled water that graduated cylinder measures 90mL is used in combination to be positioned over above-mentioned beaker
In, it is transferred in the hydrothermal reaction kettle of 100mL and is tightened after stirring evenly；Above-mentioned hydrothermal reaction kettle is positioned over Muffle furnace
In, 9h is kept the temperature at a temperature of 170 DEG C, is cooled to room temperature after reaction, carbosphere is obtained through centrifugation drying；By carbosphere plus
Enter in beaker, and distilled water appropriate is added, be configured to a concentration of 3.5% solution, weighs 120mg sodium molybdates, 250mg thiocarbamides
It is positioned in above-mentioned sample, is positioned in hydrothermal reaction kettle after stirring evenly, keep the temperature 14h at a temperature of 230 DEG C, reaction terminates
Postcooling obtains the flower-shaped MoS of micron order to room temperature after centrifugal drying2/ C microballoon composite materials, are placed in tube furnace,
1.5h is kept the temperature at a temperature of 800 DEG C, quenching treatment is carbonized to get the flower-shaped MoS of micron order2/ C microballoon composite materials.
To MoS made from embodiment 1-62/ C microballoon composite materials carry out performance detection
1, structural characterization
To MoS made from embodiment 1-62/ C microballoon composite materials carry out structural characterization, and wherein Fig. 1 and Fig. 2 are respectively real
The SEM figures for applying example 1 and embodiment 2, it can be seen from the figure that molybdenum dioxide is successfully grown in carbosphere surface.
2, Electrochemical Characterization
By MoS made from embodiment 1-62/ C microballoons composite material is assembled into button electricity as the cathode of lithium ion battery
Pond, wherein conductive agent are superconduction carbon black, and adhesive is sodium carboxymethylcellulose, and solvent is N-Methyl pyrrolidone, are stood for 24 hours
Afterwards, charge and discharge are carried out on blue electric battery test system at room temperature, wherein charging/discharging voltage window is putting for 0.001-2.5V
In electric section, charging and discharging currents 50mA/g.
Contrast test：By molybdenum disulfide not compound with carbosphere, quenched with 800 DEG C of temperature in tube furnace
1h, the cathode as lithium ion battery are assembled into button cell, and as a comparison case 1, remaining ingredient of battery and testing conditions are same as above.
1 battery performance test result of table
From upper table it will be seen that when the molybdenum disulfide compound with carbosphere is as negative material, either first circle
Specific capacity or first circle coulombic efficiency and 100 weeks capacity retention ratios have significantly compared with the molybdenum disulfide compound without carbon ball
Promoted, this is because molybdenum disulfide and carbosphere carry out it is compound after not only improve the conductivity of itself, also limit two sulphur
Change volume expansion of the molybdenum in cyclic process.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of MoS for negative electrode of lithium ion battery2/ C microballoon composite materials, which is characterized in that the composite material is by two
Molybdenum sulfide and carbosphere are combined, and the molybdenum disulfide is grown in carbosphere surface.
2. a kind of based on the MoS described in claim 1 for negative electrode of lithium ion battery2The preparation method of/C microballoon composite materials,
It is characterized by comprising the following steps：
S1, the aqueous solution for preparing saccharide compound；
S2, the aqueous solution of saccharide compound is added in hydrothermal reaction kettle, is placed in Muffle furnace and carries out hydro-thermal reaction, reaction terminates
Postcooling to room temperature, centrifugation drying obtains carbosphere；
S3, add water, stirring that sodium molybdate, thiocarbamide are added thereto into carbosphere, stirring is transferred in hydrothermal reaction kettle and carries out
Hydro-thermal reaction is cooled to room temperature after reaction, and centrifugal drying obtains MoS2/ C microballoon composite material crude products；
S4, in an inert atmosphere, by MoS2/ C microballoon composite materials carry out quenching treatment to get the flower-shaped MoS of micron order2/ C is micro-
Ball composite material.
3. the MoS according to claim 2 for negative electrode of lithium ion battery2The preparation method of/C microballoon composite materials, it is special
Sign is, in the S1, saccharide compound is any one in glucose, fructose, sucrose.
4. the MoS according to claim 2 for negative electrode of lithium ion battery2The preparation method of/C microballoon composite materials, it is special
Sign is, in the S1, the mass concentration of saccharide compound aqueous solution is 0.5-2%.
5. the preparation method of the MoS2/C microballoon composite materials according to claim 2 for negative electrode of lithium ion battery,
It is characterized in that, in the S2, hydrothermal temperature is 120-180 DEG C, reaction time 5-10h.
6. the MoS according to claim 2 for negative electrode of lithium ion battery2The preparation method of/C microballoon composite materials, it is special
Sign is, in the S3, into carbosphere plus water is configured to the solution that mass concentration is 0.5-5%.
7. the MoS according to claim 2 for negative electrode of lithium ion battery2The preparation method of/C microballoon composite materials, it is special
Sign is, in the S3, the mass ratio of sodium molybdate and thiocarbamide is 50-150：100-500.
8. the MoS according to claim 2 for negative electrode of lithium ion battery2The preparation method of/C microballoon composite materials, it is special
Sign is, in the S3, thermal response temperature is 150-240 DEG C, reaction time 10-15h.
9. the MoS according to claim 2 for negative electrode of lithium ion battery2The preparation method of/C microballoon composite materials, it is special
Sign is, in the S4, hardening heat is 300-1000 DEG C, cool time 0.5-5h.
10. the MoS according to claim 2 for negative electrode of lithium ion battery2The preparation method of/C microballoon composite materials,
It is characterized in that, in the S4, quenching is tube furnace with device.
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| CN115367801A (en) * | 2022-07-07 | 2022-11-22 | 河南科技大学 | Near-spherical molybdenum disulfide-carbon composite material for lithium ion battery cathode and preparation method thereof |
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